在Pirkle型手性固定相ULMO上同时分离氟布芬及其非对映异构体代谢产物。

Enantiomer Pub Date : 2000-01-01
G Uray, B Kosjek
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引用次数: 0

摘要

采用正相高效液相色谱法,4 -(2′,4′-二氟联苯基-4-基)-4-氧-2-甲基丁酸(氟布芬)的对映体可在whelk - 01 (α = 1.34)、ULMO (α = 1.08)和Chiralcel ODH (α = 1.33)手性固定相上分离得到。(R,R/S,S)-和(R,S/S,R)-5-(2',4'-二氟联苯-4-基)-3-甲基呋喃-2- 1,4 -羟基代谢物的内酯只能在ULMO上完全分离。在同一CSP上,该4-(2′,4′-二氟联苯-4-基)-4-羟基-2-甲基丁酸可以部分分离(α = 1.06和1.12)。通过NOE实验确定了代谢产物的绝对构型。
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Simultaneous enantioseparation of flobufen and its diastereomeric metabolites on ULMO, a Pirkle type chiral stationary phase.

Using normal-phase HPLC, the enantiomers of 4-(2',4'-difluorobiphenyl-4-yl)-4-oxo-2-methylbutanoic acid (flobufen) could be separated on Whelk-O1 (alpha = 1.34), ULMO (alpha = 1.08) and Chiralcel ODH (alpha = 1.33) chiral stationary phases. (R,R/S,S)- and (R,S/S,R)-5-(2',4'-difluorobiphenyl-4-yl)-3-methylfuran-2-one, the lactone of the 4-hydroxy metabolite could be completely separated on ULMO only. On the same CSP this 4-(2',4'-difluorobiphenyl-4-yl)-4-hydroxy-2-methylbutanoic acid could be separated in part (alpha = 1.06 and 1.12). Absolute configuration of the metabolites was established by NOE experiments.

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